JPS6319479B2 - - Google Patents

Info

Publication number
JPS6319479B2
JPS6319479B2 JP87779A JP87779A JPS6319479B2 JP S6319479 B2 JPS6319479 B2 JP S6319479B2 JP 87779 A JP87779 A JP 87779A JP 87779 A JP87779 A JP 87779A JP S6319479 B2 JPS6319479 B2 JP S6319479B2
Authority
JP
Japan
Prior art keywords
urea
weight
parts
fertilizer
hexamethylenetetramine
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
JP87779A
Other languages
Japanese (ja)
Other versions
JPS5595697A (en
Inventor
Osamu Akizuki
Kihachiro Kodama
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Chemical Co Ltd
Original Assignee
Sumitomo Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Chemical Co Ltd filed Critical Sumitomo Chemical Co Ltd
Priority to JP87779A priority Critical patent/JPS5595697A/en
Publication of JPS5595697A publication Critical patent/JPS5595697A/en
Publication of JPS6319479B2 publication Critical patent/JPS6319479B2/ja
Granted legal-status Critical Current

Links

Description

【発明の詳細な説明】[Detailed description of the invention]

本発明は尿素―ホルムアルデヒド縮合物を含有
する緩効性粒状複合肥料の製造方法に関する。 窒素肥料として肥効の高い尿素―ホルムアルデ
ヒド縮合物は工業的にはホルムアルデヒド水溶液
に定められた量の尿素を混入し、アルカリ性下、
温度30〜80℃の条件でメチロール化反応を行なわ
せ、得られたメチロール尿素液を酸性下、温度30
〜100℃の条件でメチレン化反応をさせる方法に
よつて得られる。 これらの方法によつて得られた尿素―ホルムア
ルデヒド縮合物を粒状の複合肥料とする場合、こ
れを粉末にして、これに硫安、尿素、リン安、塩
化加里等の肥料物質を混合して造粒機に導入し、
結合剤として水又は必要に応じて酸、塩基、可溶
性塩類等を添加して造粒し乾燥することによつて
製造されている。 このような方法で製造された尿素―ホルムアル
デヒド縮合物を含有する緩効性粒状複合肥料は高
価な尿素―ホルムアルデヒド縮合物を使用するた
め経済的に不利であり、また造粒性が悪いという
欠点があつた。 本発明者らはこれらの欠点を解決するため種種
検討した結果、複合造粒肥料を製造する造粒機内
に尿素とヘキサメチレンテトラミンを共存させ酸
性下で複合肥料を造粒することにより、下式の反
応が起こり別途に尿素―ホルムアルデヒド縮合物
を添加することなく尿素―ホルムアルデヒド縮合
物を含有する複合造粒肥料を製造することができ
ることを見出し、本発明に到達した。
The present invention relates to a method for producing a slow-release granular composite fertilizer containing a urea-formaldehyde condensate. Industrially, the urea-formaldehyde condensate, which is highly effective as a nitrogen fertilizer, is produced by mixing a specified amount of urea into an aqueous formaldehyde solution and then treating it under alkaline conditions.
The methylolation reaction was carried out at a temperature of 30 to 80℃, and the resulting methylolurea solution was heated under acidic conditions at a temperature of 30℃.
It is obtained by a method of carrying out a methylenation reaction at a temperature of ~100°C. When the urea-formaldehyde condensate obtained by these methods is made into a granular composite fertilizer, it is powdered, mixed with fertilizer substances such as ammonium sulfate, urea, ammonium phosphorous, potassium chloride, etc., and granulated. Introduced into the machine,
It is produced by adding water or, if necessary, acids, bases, soluble salts, etc. as a binder, granulating it, and drying it. Slow-release granular composite fertilizers containing urea-formaldehyde condensates produced by this method are economically disadvantageous because they use expensive urea-formaldehyde condensates, and they also have the disadvantage of poor granulation properties. It was hot. In order to solve these drawbacks, the present inventors investigated various types of fertilizers, and found that by making urea and hexamethylenetetramine coexist in a granulator for producing a composite granulated fertilizer and granulating the composite fertilizer under acidic conditions, the following formula was developed. The inventors have discovered that a composite granulated fertilizer containing a urea-formaldehyde condensate can be produced without separately adding a urea-formaldehyde condensate through the following reaction, and have thus arrived at the present invention.

【表】 即ち本発明はヘキサメチレンテトラミンを尿素
を含有する肥料物質と混合し、無機酸の存在下で
造粒することからなる尿素―ホルムアルデヒド縮
合物を含有する緩効性粒状複合肥料の製造方法で
ある。 以下本発明について詳述する。 本発明が対象とする緩効性粒状複合肥料として
は窒素―リン酸系又は窒素―カリ系の二成分系お
よび窒素―リン酸―カリ系の三成分系である。 本発明の緩効性粒状複合肥料中の全窒素成分に
しめる緩効性窒素成分の比率の上限は反応式(1)、
(2)、(3)からも明らかなごとく、使用する無機酸の
種数および添加量、即ちヘキサメチレンテトラミ
ンの分解で副生する硫安、リン安等の副生量によ
り決まるが、通常これらの混合系に速効性の窒素
成分が加えられるので実験はこれら上限値以下の
範囲になる。 本発明において用いられる肥料物質としては、
硫安、尿素等の窒素系、リン酸―アンモニウム、
リン酸二アンモニウム等のリン酸系および塩化加
里、硫酸カリ等のカリ系物質が主として用いられ
るが、更にマグネシウム、銅、マンガン、ホウ素
等の微量要素成分を添加することも可能である。 これら肥料物質は通常粉状品で用いられるが、
場合によつては濃厚な水溶液又はスラリー等で用
いることもできる。 本発明において用いられるヘキサメチレンテト
ラミンは工業用の粉状品が好ましい。ヘキサメチ
レンテトラミンに対する尿素の添加量はモル比で
7〜18の範囲が好ましい。ヘキサメチレンテトラ
ミンに対する尿素の添加量がこれ以上の場合は緩
効性の効果が小さくなり好ましくなく、又これ以
下の場合は尿素―ホルムアルデヒド縮合物の高重
合化が進行し、溶解性が悪くなるので好ましくな
い。 造粒時に存在させる無機酸としては、例えば硫
酸、リン酸などの鉱酸が挙げられ、これらは通常
70〜98重量%硫酸又は30〜55重量%リン酸水溶液
で使用される。 これら無機酸は造粒剤として作用するほか、一
部はヘキサメチレンテトラミンの分解剤および尿
素とホルムアルデヒドとの縮合剤として作用し、
過剰に存在する無機酸は造粒時アンモニアガスを
添加することにより中和されて最終的には硫安又
はリン安等になる。 本発明において使用される造粒機は通常用いら
れている造粒機、例えば皿型造粒機、ドラム型造
粒機等である。 造粒温度は100℃以下が好ましく、温度が100℃
以上になるとホルムアルデヒドが未反応のまま蒸
発し、有効な反応が行なわれないので好ましくな
い。 造粒時間は特に限定されないが、通常5〜10分
間位で行なわれる。 上記方法により造粒したのち、通常の乾燥機で
一定時間乾燥を行ない、最後に分級したのち製品
とすることができる。 以上述べたごとく、本発明方法によつて造粒機
内で尿素―ホルムアルデヒド縮合物を生成させな
がら、造粒性の高い複合肥料が造粒できるので、
高価な尿素―ホルムアルデヒド縮合物を別途に合
成する必要がなく、従来のプロセスがそのまま使
用することができるので工業的に有用な方法であ
る。 以下本発明を実施例により更に説明するが、本
発明はこれら実施例により何ら制限されるもので
はない。 実施例 直径0.6m、深さ0.15mの皿型造粒機に、ヘキサ
メチレンテトラミンの分解によつて生成するホル
ムアルデヒドと尿素のモル比が1:2となるよう
に、ヘキサメチレンテトラミン(純度98.7%)17
重量部と尿素88重量部、更に硫安(N:21%)82
重量部、塩化加里(K2O:61%)208重量部、オ
リビンサンド151重量部を供給混合し、別途湿式
リン酸(P2O5:36%、H2SO4:5%)578重量部
をアンモニアガス85重量部で中和して得た燐安ス
ラリーを前記混合物に添加し、次にこの混合物を
撹拌しながら98%硫酸36重量部をスプレーで添加
し、同時にアンモニアガス17重量部を添加して5
分間で造粒した。造粒機内の温度は約70℃迄上昇
し、造粒物の水分は3.2%であつた。これを98℃
で1時間乾燥し、乾燥後分級して6〜12メツシユ
の製品725重量部を得た。得られた製品の品質は
下記のとおりであつた。
[Table] That is, the present invention is a method for producing a slow-release granular composite fertilizer containing a urea-formaldehyde condensate, which comprises mixing hexamethylenetetramine with a fertilizer substance containing urea and granulating it in the presence of an inorganic acid. It is. The present invention will be explained in detail below. Slow-release granular compound fertilizers targeted by the present invention include binary nitrogen-phosphoric acid or nitrogen-potassium systems and ternary nitrogen-phosphoric acid-potassium systems. The upper limit of the ratio of the slow-release nitrogen component to the total nitrogen component in the slow-release granular compound fertilizer of the present invention is determined by the reaction formula (1):
As is clear from (2) and (3), it is determined by the number of inorganic acids used and the amount added, that is, the amount of by-products such as ammonium sulfate and ammonium phosphorous produced by the decomposition of hexamethylenetetramine. Since a fast-acting nitrogen component is added to the mixed system, the experiments will be in the range below these upper limits. Fertilizer substances used in the present invention include:
Nitrogen-based materials such as ammonium sulfate and urea, ammonium phosphate,
Phosphate-based substances such as diammonium phosphate and potassium-based substances such as potassium chloride and potassium sulfate are mainly used, but it is also possible to further add trace elements such as magnesium, copper, manganese, and boron. These fertilizer substances are usually used in powder form;
Depending on the case, it can also be used in the form of a concentrated aqueous solution or slurry. The hexamethylenetetramine used in the present invention is preferably an industrial powder product. The amount of urea added to hexamethylenetetramine is preferably in the range of 7 to 18 in terms of molar ratio. If the amount of urea added to hexamethylenetetramine is more than this, the slow-release effect will be reduced, which is undesirable, and if it is less than this, high polymerization of the urea-formaldehyde condensate will progress, resulting in poor solubility. Undesirable. Examples of inorganic acids to be present during granulation include mineral acids such as sulfuric acid and phosphoric acid, which are usually
Used in an aqueous solution of 70-98% by weight sulfuric acid or 30-55% by weight phosphoric acid. In addition to acting as a granulating agent, some of these inorganic acids also act as a decomposing agent for hexamethylenetetramine and a condensing agent for urea and formaldehyde.
Excessive inorganic acid is neutralized by adding ammonia gas during granulation and ultimately becomes ammonium sulfate or ammonium phosphorus. The granulator used in the present invention is a commonly used granulator, such as a dish-type granulator or a drum-type granulator. The granulation temperature is preferably 100℃ or less, and the temperature is 100℃
If the reaction temperature exceeds that level, the formaldehyde will evaporate unreacted and no effective reaction will take place, which is not preferable. The granulation time is not particularly limited, but it is usually carried out for about 5 to 10 minutes. After granulation by the above method, it is dried for a certain period of time in an ordinary dryer, and finally classified, and then a product can be obtained. As described above, by the method of the present invention, a compound fertilizer with high granulability can be granulated while generating a urea-formaldehyde condensate in the granulator.
It is an industrially useful method because there is no need to separately synthesize an expensive urea-formaldehyde condensate, and conventional processes can be used as they are. The present invention will be further explained below with reference to Examples, but the present invention is not limited to these Examples in any way. Example Hexamethylenetetramine (purity 98.7%) was placed in a dish-shaped granulator with a diameter of 0.6m and a depth of 0.15m so that the molar ratio of formaldehyde and urea produced by the decomposition of hexamethylenetetramine was 1:2. )17
parts by weight and 88 parts by weight of urea, and further ammonium sulfate (N: 21%) 82
Parts by weight, 208 parts by weight of potassium chloride (K 2 O: 61%) and 151 parts by weight of olivine sand were supplied and mixed, and separately 578 parts by weight of wet phosphoric acid (P 2 O 5 : 36%, H 2 SO 4 : 5%) were added. A phosphoric ammonium slurry obtained by neutralizing 1.0 parts with 85 parts by weight of ammonia gas was added to the mixture, and then, while stirring the mixture, 36 parts by weight of 98% sulfuric acid was added by spray, and at the same time 17 parts by weight of ammonia gas was added to the mixture. Add 5
Granulated in minutes. The temperature inside the granulator rose to about 70°C, and the moisture content of the granulate was 3.2%. This is 98℃
After drying for 1 hour, the mixture was classified to obtain 725 parts by weight of a product with 6 to 12 meshes. The quality of the obtained product was as follows.

【表】 上記結果より緩効性窒素に相当する冷水不溶性
窒素および全ホルムアルデヒド量は後述する別途
尿素―ホルムアルデヒド縮合物を用いた比較例と
ほぼ同じ結果を示し、又製品収率は比較例に比べ
て著しく良いことより造粒性がすぐれていること
が判る。 比較例 ヘキサメチレンテトラミン17重量部と尿素88重
量部の代りに、尿素―ホルムアルデヒド縮合物
(N:40.4%)を100重量部用いたこと、オリビン
サンド151重量部を149重量部にしたこと、リン安
スラリーの調製に用いたアンモニアガスを85重量
部から93重量部にしたこと以外は実施例と同様の
方法で造粒した。 造粒機内の温度は約70℃迄上昇し、造粒物の水
分は3.0%であつた。これを98℃で1時間乾燥し、
乾燥後分級して6〜12メツシユの製品468重量部
を得た。
[Table] From the above results, the amounts of cold water-insoluble nitrogen and total formaldehyde, which correspond to slow-release nitrogen, are almost the same as those of the comparative example using a urea-formaldehyde condensate, which will be described later, and the product yield is also higher than that of the comparative example. It can be seen that the granulation properties are excellent. Comparative example: 100 parts by weight of urea-formaldehyde condensate (N: 40.4%) was used instead of 17 parts by weight of hexamethylenetetramine and 88 parts by weight of urea, 149 parts by weight was changed from 151 parts by weight of olivine sand, phosphorus Granulation was carried out in the same manner as in Example except that the amount of ammonia gas used to prepare the cheap slurry was changed from 85 parts by weight to 93 parts by weight. The temperature inside the granulator rose to about 70°C, and the moisture content of the granules was 3.0%. Dry this at 98℃ for 1 hour,
After drying, it was classified to obtain 468 parts by weight of a product with 6 to 12 meshes.

【表】【table】

Claims (1)

【特許請求の範囲】[Claims] 1 ヘキサメチレンテトラミンを尿素を含有する
肥料物質と混合し、無機酸の存在下で造粒するこ
とを特徴とする尿素―ホルムアルデヒド縮合物を
含有する緩効性粒状複合肥料の製造方法。
1. A method for producing a slow-release granular composite fertilizer containing a urea-formaldehyde condensate, which comprises mixing hexamethylenetetramine with a fertilizer substance containing urea and granulating the mixture in the presence of an inorganic acid.
JP87779A 1979-01-05 1979-01-05 Manufacture of slowwacting granular composite fertilizer containing ureaaformaldehyde condensates Granted JPS5595697A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP87779A JPS5595697A (en) 1979-01-05 1979-01-05 Manufacture of slowwacting granular composite fertilizer containing ureaaformaldehyde condensates

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP87779A JPS5595697A (en) 1979-01-05 1979-01-05 Manufacture of slowwacting granular composite fertilizer containing ureaaformaldehyde condensates

Publications (2)

Publication Number Publication Date
JPS5595697A JPS5595697A (en) 1980-07-21
JPS6319479B2 true JPS6319479B2 (en) 1988-04-22

Family

ID=11485894

Family Applications (1)

Application Number Title Priority Date Filing Date
JP87779A Granted JPS5595697A (en) 1979-01-05 1979-01-05 Manufacture of slowwacting granular composite fertilizer containing ureaaformaldehyde condensates

Country Status (1)

Country Link
JP (1) JPS5595697A (en)

Also Published As

Publication number Publication date
JPS5595697A (en) 1980-07-21

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